WO2016199829A1 - Composition de résine, film, écran tactile et dispositif d'affichage - Google Patents

Composition de résine, film, écran tactile et dispositif d'affichage Download PDF

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Publication number
WO2016199829A1
WO2016199829A1 PCT/JP2016/067145 JP2016067145W WO2016199829A1 WO 2016199829 A1 WO2016199829 A1 WO 2016199829A1 JP 2016067145 W JP2016067145 W JP 2016067145W WO 2016199829 A1 WO2016199829 A1 WO 2016199829A1
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resin
film
mass
layer
meth
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PCT/JP2016/067145
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English (en)
Japanese (ja)
Inventor
一喜 大松
美保 大関
山下　恭弘
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住友化学株式会社
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Priority to JP2017523681A priority Critical patent/JP6374610B2/ja
Publication of WO2016199829A1 publication Critical patent/WO2016199829A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/16—Homopolymers or copolymers or vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters

Definitions

  • the present invention relates to a resin composition, a film, and a touch sensor panel.
  • touch sensor panels have been used for smartphones, portable game machines, audio players, tablet terminals, and the like.
  • a film having conductivity and transparency is used as a protective sheet, and as such a film, for example, a film containing methacrylic resin and polyvinylidene fluoride is known ( Patent Document 1).
  • the inventors of the present invention have intensively studied a film for a touch sensor panel that has a high relative dielectric constant and can maintain transparency even when used for a long time.
  • vinylidene fluoride used for a resin composition constituting the film is used.
  • the present inventors have found that the contents of the structural unit derived from vinylidene fluoride in the resin and the structural unit derived from hexafluoropropylene greatly affect the durability, and completed the present invention.
  • a resin composition comprising a (meth) acrylic resin and a vinylidene fluoride resin, wherein 45 to 60 parts by mass of the (meth) acrylic resin per 100 parts by mass of the total amount of the (meth) acrylic resin and the vinylidene fluoride resin And 40 to 55 parts by mass of a vinylidene fluoride resin, the vinylidene fluoride resin having a total structural unit of 100% by mass and a structural unit derived from vinylidene fluoride of 65 to 90% by mass, hexafluoropropylene
  • a resin composition which is a vinylidene fluoride-hexafluoropropylene copolymer containing 10 to 35% by mass of a structural unit derived from [2]
  • the resin composition according to [1], wherein the (meth) acrylic resin is the following resin (a1) or (a2); (A1) methyl methacrylate homopolymer, (A2)
  • [6] A film formed from the resin composition according to any one of [1] to [5]; [7] A film containing a (meth) acrylic resin and a vinylidene fluoride resin, wherein the vinylidene fluoride resin has a structural unit of 65 to 90% by mass derived from vinylidene fluoride with 100% by mass as a whole. And a vinylidene fluoride-hexafluoropropylene copolymer containing 10 to 35% by mass of a structural unit derived from hexafluoropropylene, The film has a relative dielectric constant of 4.0 or more and a haze of 2% or less after exposure for 120 hours at 60 ° C. in an environment with a relative humidity of 90%.
  • thermoplastic resin layer includes a plurality of thermoplastic resin layers and is disposed on both surfaces of the film;
  • thermoplastic resin layer contains 50 parts by mass or more of (meth) acrylic resin per 100 parts by mass of the thermoplastic resin constituting the thermoplastic resin layer.
  • a third laminate that is a layer that is disposed on and imparts at least one function; [17] A touch sensor panel including the film according to any one of [6] to [8]; [18] A touch including the first stacked body according to [9], the second stacked body according to any one of [10] to [15], or the third stacked body according to [17]. Sensor panel; [19] A display device comprising the film according to any one of [6] to [8]; [20] Display including the first laminate according to [9], the second laminate according to any one of [10] to [15], or the third laminate according to [17] apparatus.
  • the film formed from the resin composition of the present invention is useful as a window sheet for a touch sensor panel because it has a high relative dielectric constant and can maintain transparency even when used for a long time.
  • (meth) acrylic resin used in the present invention examples include a homopolymer of (meth) acrylic monomers such as (meth) acrylic acid ester and (meth) acrylonitrile, or two or more types of copolymers; Examples include copolymers of acrylic monomers and other monomers.
  • (meth) acryl means “acryl” or “methacryl”.
  • a methacrylic resin is a polymer obtained by polymerizing a monomer mainly composed of a methacrylic acid ester (alkyl methacrylate).
  • a methacrylic acid ester homopolymer (polyalkyl methacrylate) and a methacrylic acid ester examples thereof include a polymer and a copolymer of 50% by mass or more of a methacrylic acid ester and a monomer other than 50% by mass of a methacrylic acid ester.
  • the methacrylic acid ester is preferably 70% by mass or more and the monomer other than the methacrylic acid ester with respect to the total monomer amount of 100% by mass. Is 30% by mass or less, more preferably 90% by mass or more of methacrylic acid ester and 10% by mass or less of monomers other than methacrylic acid ester.
  • Examples of monomers other than methacrylic acid esters include acrylic acid esters and monofunctional monomers having one polymerizable carbon-carbon double bond in the molecule.
  • Monofunctional monomers include, for example, styrene monomers such as styrene, ⁇ -methylstyrene and vinyltoluene; alkenyl cyanides such as acrylonitrile and methacrylonitrile; acrylic acid; methacrylic acid; maleic anhydride; phenylmaleimide N-substituted maleimides such as cyclohexylmaleimide and methylmaleimide; From the viewpoint of heat resistance, a lactone ring structure, a glutaric anhydride structure, or a glutarimide structure is present in the molecular chain of the (meth) acrylic resin (also referred to as the main skeleton or main chain in the (meth) acrylic resin). It may be introduced.
  • styrene monomers such as styrene, ⁇ -methylstyrene and vinyltoluene
  • alkenyl cyanides such as acrylonitrile and methacrylonitrile
  • the (meth) acrylic resin is preferably the following resin (a1) or (a2).
  • the total amount of the structural unit derived from methyl methacrylate and at least one structural unit derived from the (meth) acrylic acid ester represented by the formula (1) is 100% by mass. It is preferable.
  • Copolymer containing (Wherein R 1 represents a hydrogen atom or a methyl group, when R 1 is a hydrogen atom, R 2 represents an alkyl group having 1 to 8 carbon atoms, and when R 1 is a methyl group, R 2 represents 2 to 2 carbon atoms) Represents an alkyl group of 8).
  • R 1 is a hydrogen atom
  • the alkyl group having 1 to 8 carbon atoms represented by R 2 is methyl group, ethyl group, propyl group, isopropyl group, butyl group, sec-butyl group, tert- A butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group, and the like.
  • Examples of the alkyl group having 2 to 8 carbon atoms represented by R 2 when R 1 is a methyl group include an ethyl group, a propyl group, Examples include isopropyl group, butyl group, sec-butyl group, tert-butyl group, pentyl group, hexyl group, heptyl group, octyl group and the like.
  • the (meth) acrylic acid ester represented by the formula (1) is preferably methyl acrylate or ethyl acrylate, and more preferably methyl acrylate.
  • the (meth) acrylic resin has a melt mass flow rate at 230 ° C. (hereinafter sometimes referred to as MFR) measured at a load of 3.8 kg in accordance with JIS K7210, usually 0.1 to 20 g / 10 minutes, preferably Is 0.2 to 5 g / 10 min, and more preferably 0.5 to 3 g / 10 min.
  • MFR melt mass flow rate measured at a load of 3.8 kg in accordance with JIS K7210
  • the (meth) acrylic resin preferably has a weight average molecular weight (hereinafter sometimes referred to as Mw) determined by GPC measurement of 70,000 to 300,000, more preferably 100,000 to 250,000. 120,000 to 250,000 is more preferable, and 150,000 to 200,000 is more preferable.
  • Mw weight average molecular weight
  • the (meth) acrylic resin preferably has a Vicat softening temperature (hereinafter sometimes referred to as VST) measured according to JIS K7206 of 90 ° C. or higher, more preferably 100 ° C. or higher. Preferably, it is 102 ° C. or higher.
  • VST Vicat softening temperature
  • the VST of the (meth) acrylic resin can be appropriately set by adjusting the type and ratio of the monomer or the molecular weight of the (meth) acrylic resin.
  • (Meth) acrylic resin can be prepared by polymerizing the monomer component by a method such as suspension polymerization or bulk polymerization.
  • MFR, Mw, VST, etc. of (meth) acrylic resin can be adjusted to a preferable range by adding a suitable chain transfer agent. What is necessary is just to determine the addition amount of a chain transfer agent suitably according to the kind of monomer, its ratio, the characteristic calculated
  • the (meth) acrylic resin preferably has a low alkali metal content. The content of the alkali metal can be adjusted by reducing the amount of the compound containing the alkali metal during the polymerization, or increasing the washing step after the polymerization to remove the compound containing the alkali metal.
  • (Meth) acrylic resin may be a commercially available product.
  • examples of preferable commercial products include “SUMIPEX (registered trademark) MM” manufactured by Sumitomo Chemical Co., Ltd.
  • the vinylidene fluoride resin used in the present invention has a structural unit of 65 to 90% by mass derived from vinylidene fluoride, based on 100% by mass of all the structural units of the vinylidene fluoride resin, A vinylidene fluoride-hexafluoropropylene copolymer containing 10 to 35% by mass of a structural unit derived from hexafluoropropylene.
  • the vinylidene fluoride resin is a group consisting of trifluoroethylene, tetrafluoroethylene, chlorotrifluoroethylene, perfluoroalkyl vinyl ether and ethylene in addition to the structural unit derived from vinylidene fluoride and the structural unit derived from hexafluoropropylene.
  • a structural unit derived from at least one monomer selected from may be included.
  • the content of the structural unit derived from hexafluoropropylene contained in the vinylidene fluoride-hexafluoropropylene copolymer is preferably 10 to 30% by mass, more preferably 10 to 25% by mass.
  • the content of the structural unit derived from vinylidene fluoride contained in the vinylidene fluoride-hexafluoropropylene copolymer is preferably 70 to 90% by mass, more preferably 75 to 90% by mass.
  • the total amount of the content of the structural unit derived from vinylidene fluoride and the content of the structural unit derived from hexafluoropropylene in 100% by mass of the vinylidene fluoride resin is 100% by mass.
  • the structural unit derived from these monomers is preferably 25% by mass or less, more preferably 20% by mass or less, and even more preferably 15% by mass or less, based on 100% by mass of all structural units of the vinylidene fluoride resin. .
  • the vinylidene fluoride resin usually has a melt mass flow rate (MFR) at 230 ° C. of 0.1 to 40 g / 10 minutes measured under a load of 3.8 kg in accordance with JIS K7210.
  • the upper limit of the MFR is preferably 35 g / 10 minutes, more preferably 30 g / 10 minutes, still more preferably 25 g / 10 minutes, and even more preferably 20 g / 10 minutes.
  • the upper limit of the MFR is preferably 0.2 g / 10 minutes, and more preferably 0.5 g / 10 minutes. If the MFR of the vinylidene fluoride resin is too large, the transparency tends to decrease when the resulting film is used for a long period of time. If the MFR of the vinylidene fluoride resin is too small, the film formability tends to decrease. .
  • the vinylidene fluoride resin preferably has a weight average molecular weight (Mw) determined by GPC measurement of 100,000 to 500,000, more preferably 150,000 to 450,000, and 200,000 to 450. More preferably, it is 1,000.
  • Mw weight average molecular weight
  • the vinylidene fluoride resin is industrially produced by a suspension polymerization method or an emulsion polymerization method.
  • a suspension polymerization method water is used as a medium, the monomer is dispersed as droplets in the medium using a dispersant, and an organic peroxide dissolved in the monomer is polymerized as a polymerization initiator, whereby 100 to 100% is obtained.
  • a 300 ⁇ m granular polymer is obtained.
  • Suspension polymers are preferred because they have a simpler manufacturing process, better powder handling, and do not contain an emulsifier or salting-out agent containing an alkali metal unlike emulsion polymers.
  • the amount of alkali metal contained in the vinylidene fluoride resin is preferably 1 ppm or less.
  • a commercially available vinylidene fluoride resin may be used.
  • examples of preferable commercial products include K #, Kureha's “KF Polymer (registered trademark)” T # 2950, and Solvay's “SOLEF®” 21508.
  • the resin composition of the present invention contains 45 to 60 parts by mass of (meth) acrylic resin and 40 to 55 parts by mass of vinylidene fluoride resin per 100 parts by mass of the total amount of (meth) acrylic resin and vinylidene fluoride resin. It is a waste.
  • the total content of the (meth) acrylic resin and the vinylidene fluoride resin in 100% by mass of the resin composition is preferably 90% by mass or more, and more preferably 95% by mass or more.
  • the resin composition may contain a vinylidene fluoride resin other than the vinylidene fluoride-hexafluoropropylene copolymer, and the content thereof is preferably 10% by mass or less in 100% by mass of the resin composition.
  • vinylidene fluoride resins other than vinylidene fluoride-hexafluoropropylene copolymers are all commercially available, and Kureha's “KF Polymer (registered trademark)” T # 1300, T # 1100, T Examples include # 1000, T # 850, W # 850, W # 1000, W # 1100, and W # 1300, “SOLEF (registered trademark)” 6012, 6010, 6008, and 31508 manufactured by Solvay.
  • alkali metal contained in the resin composition examples include sodium and potassium derived from the remaining emulsifier when using the vinylidene fluoride resin obtained by the above emulsion polymerization.
  • the range is usually 50 ppm or less, preferably 30 ppm or less, more preferably 10 ppm or less, and it is further preferred that it is not substantially contained.
  • the content of alkali metal in the resin composition can be determined by, for example, inductively coupled plasma mass spectrometry (ICP / MS).
  • additives may be added to the resin composition of the present invention as long as the effects of the present invention are not impaired.
  • additives include stabilizers, antioxidants, ultraviolet absorbers, light stabilizers, colorants, foaming agents, lubricants, mold release agents, antistatic agents, flame retardants, polymerization inhibitors, flame retardant aids, Examples include coloring agents such as reinforcing agents, nucleating agents, and bluing agents.
  • Examples of the colorant include compounds having an anthraquinone skeleton, compounds having a phthalocyanine skeleton, and the like. Among these, a compound having an anthraquinone skeleton is preferable from the viewpoint of heat resistance.
  • a bluing agent When a bluing agent is used as a colorant, its content is 0.01 to 5 ppm, preferably 0.05 to 4 ppm, more preferably 0.1 to 3 ppm.
  • a known bluing agent can be appropriately used.
  • the bluing agent for example, Macrolex (registered trademark) Blue RR (manufactured by Bayer), Macrolex (registered trademark) Blue 3R (manufactured by Bayer), Sumiplast (registered trademark) Violet B (Sumi) Chemical Chemtex) and Polysynthrene (registered trademark) Blue RLS (Clariant).
  • additives may be present in the resin composition of the present invention, and may be contained in any component of the (meth) acrylic resin or vinylidene fluoride resin. May be added during melt-kneading with vinylidene fluoride resin, may be added after melt-kneading between (meth) acrylic resin and vinylidene fluoride resin, or added when producing a film using a resin composition May be.
  • the resin composition of the present invention is usually obtained by kneading a (meth) acrylic resin and a vinylidene fluoride resin.
  • kneading can be performed, for example, by a method including a step of melt-kneading at a shear rate of 10 to 1000 / second at a temperature of 150 to 350 ° C.
  • the resin may not melt.
  • the resin may be thermally decomposed.
  • the shear rate at the time of melt kneading is less than 10 / second, the kneading may not be sufficiently performed.
  • the shear rate during melt-kneading exceeds 1000 / second, the resin may be decomposed.
  • the melt-kneading is preferably performed at a temperature of 180 to 300 ° C., more preferably 200 to 300 ° C., preferably 20 to 700 / second, and more. Preferably, it is carried out at a shear rate of 30 to 500 / sec.
  • an ordinary mixer or kneader can be used as an apparatus used for melt kneading.
  • Specific examples include a single-screw kneader, a twin-screw kneader, a multi-screw extruder, a Henschel mixer, a Banbury mixer, a kneader, and a roll mill.
  • a high shearing device or the like may be used.
  • the film of the present invention is formed from the resin composition of the present invention.
  • Such a film preferably has a thickness of 100 to 2000 ⁇ m, more preferably 200 to 1500 ⁇ m.
  • the film of the present invention can suppress whitening of the film that occurs in a high temperature and high humidity environment.
  • the haze is preferably 1.8% or less, more preferably 1.5% or less. It shows that whitening of a film
  • membrane is suppressed more so that a value is small.
  • the amount of change in haze before and after exposure for a long time in a high temperature and high humidity environment is preferably 10 points or less, more preferably 5 points or less, and even more preferably 1 point or less. And more preferably 0.5 points or less.
  • One embodiment of the laminate of the present invention comprises the above-described film and a thermoplastic resin layer (second laminate).
  • a laminate is excellent in heat resistance and surface hardness.
  • the thermoplastic resin layer only needs to be laminated on at least one surface of the film formed from the resin composition of the present invention, and does not necessarily need to be in contact with the film, and is laminated via another layer. Also good.
  • the thermoplastic resin layer is preferably laminated in contact with the film made of the resin composition of the present invention. From the viewpoint of maintaining the shape of the film, the laminate preferably includes a thermoplastic resin layer on both sides of the film.
  • the laminate may further include a coating layer described later (third laminate).
  • the thickness of the thermoplastic resin layer is preferably 10 to 200 ⁇ m, and more preferably 50 to 150 ⁇ m.
  • the thickness and composition of each thermoplastic resin layer may be the same or different from each other, but from the viewpoint of maintaining the shape of the film, Are preferably the same.
  • the pencil hardness measured according to JIS K5600-5-4 of the thermoplastic resin layer is preferably HB or more, more preferably F or more, and further preferably H or more.
  • the Vicat softening temperature of the thermoplastic resin layer measured according to JIS K7206 is preferably 100 to 150 ° C.
  • the thermoplastic resin layer can be selected from one or more types of (meth) acrylic resins or one or more types of thermoplastic resins other than (meth) acrylic resins. From these resins, one or more types of thermoplastic resins can be used alone or in combination.
  • the thermoplastic resin layer can have a single layer configuration or a configuration in which a plurality of layers are laminated.
  • the (meth) acrylic resin of the thermoplastic resin layer a resin having the same primary structure as that of the (meth) acrylic resin contained in the resin composition of the present invention can be used.
  • Methacrylic acid resin a copolymer composed of a structural unit derived from methyl methacrylate and a structural unit derived from methacrylic acid, or a structural unit derived from styrene, a structural unit derived from maleic anhydride, and methacrylic acid
  • a terpolymer composed of a structural unit derived from methyl can be used.
  • the weight average molecular weight (Mw) of the (meth) acrylic resin is preferably 50,000 to 300,000, and more preferably 70,000 to 250,000.
  • the (meth) acrylic resin contained in the thermoplastic resin layer includes the (meth) acrylic resin contained in the resin composition forming the film They may be the same or different.
  • thermoplastic resins other than (meth) acrylic resins carbonate resins, cycloolefin resins, ethylene terephthalate resins, styrene resins, methyl methacrylate-styrene resins, acrylonitrile-styrene resins, ABS resins, etc. should be used. Can do.
  • the thermoplastic resin other than the (meth) acrylic resin preferably has a Vicat softening temperature of 115 ° C. or higher, more preferably 117 ° C. or higher, more preferably 120 ° C. or higher, from the viewpoint of heat resistance. More preferably it is.
  • the carbonate resin is a polycarbonate resin.
  • the polycarbonate resin layer is formed from one or more types of polycarbonate resins or a composite resin of one or more types of polycarbonate resins and one or more types of thermoplastic resins. Can do.
  • These polycarbonate resins are melt volume rate measured at a temperature of 300 ° C. and a load 1.2 kg (hereinafter, also referred to as MVR.) Is preferably a 3 ⁇ 120cm 3/10 min. MVR is more preferably from 3 ⁇ 80cm 3/10 minutes, more preferably 4 ⁇ 40cm 3/10 minutes, deliberately preferably 10 ⁇ 40cm 3/10 minutes.
  • MVR is less than 3 cm 3/10 min, because the flowability is decreased, and tends to be difficult by molding such as melt co-extrusion, there is the appearance failure occurs. Further, the MVR exceeds 120 cm 3/10 min, mechanical properties such as strength of the polycarbonate resin layer tends to decrease. MVR can be measured under the condition of 300 ° C. under a load of 1.2 kg in accordance with JIS K 7210.
  • the polycarbonate resin is a polymer obtained by, for example, a phosgene method in which various dihydroxydiaryl compounds and phosgene are reacted, or a transesterification method in which a dihydroxydiaryl compound and a carbonic ester such as diphenyl carbonate are reacted.
  • a phosgene method in which various dihydroxydiaryl compounds and phosgene are reacted
  • a transesterification method in which a dihydroxydiaryl compound and a carbonic ester such as diphenyl carbonate are reacted.
  • Examples thereof include polycarbonate resins produced from 2,2-bis (4-hydroxyphenyl) propane (commonly called bisphenol A).
  • dihydroxydiaryl compound examples include bisphenol 4-, bis (4-hydroxyphenyl) methane, 1,1-bis (4-hydroxyphenyl) ethane, 2,2-bis (4-hydroxyphenyl) butane, 2, 2-bis (4-hydroxyphenyl) octane, bis (4-hydroxyphenyl) phenylmethane, 2,2-bis (4-hydroxyphenyl-3-methylphenyl) propane, 1,1-bis (4-hydroxy-3) -Tert-butylphenyl) propane, 2,2-bis (4-hydroxy-3-bromophenyl) propane, 2,2-bis (4-hydroxy-3,5-dibromophenyl) propane, 2,2-bis ( Bis (hydroxyaryl) alkanes such as 4-hydroxy-3,5-dichlorophenyl) propane, 1,1 Bis (hydroxyaryl) cycloalkanes such as bis (4-hydroxyphenyl) cyclopentane, 1,1-bis (4-hydroxyphenyl) cyclohexane, 4,4
  • Trihydric or higher phenols include phloroglucin, 4,6-dimethyl-2,4,6-tri- (4-hydroxyphenyl) -heptene, 2,4,6-dimethyl-2,4,6-tri- (4 -Hydroxyphenyl) -heptane, 1,3,5-tri- (4-hydroxyphenyl) -benzol, 1,1,1-tri- (4-hydroxyphenyl) -ethane and 2,2-bis- [4 4- (4,4'-dihydroxydiphenyl) -cyclohexyl] -propane and the like.
  • the polycarbonate resin layer is formed from a composite resin of one or more types of polycarbonate resin and one or more types of thermoplastic resin
  • the thermoplastic resin other than the polycarbonate resin is blended within a range that does not impair the transparency. can do.
  • this thermoplastic resin for example, a (meth) acrylic resin compatible with a polycarbonate resin is preferable, and a methacrylic resin having an aromatic ring or a cycloolefin in its structure is more preferable.
  • the polycarbonate resin contains such a tacryl resin, the surface hardness of the obtained polycarbonate resin layer can be made higher than when the polycarbonate resin is formed from the polycarbonate resin alone.
  • Polycarbonate resins other than the above polycarbonate resins include polycarbonates synthesized from isosorbite and aromatic diols.
  • An example is “DURABIO (registered trademark)” manufactured by Mitsubishi Chemical.
  • the polycarbonate resin includes a release agent, an ultraviolet absorber, a dye, a pigment, a polymerization inhibitor, an antioxidant, a flame retardant, a reinforcing agent and other additives, a polymer other than the polycarbonate resin, and the like. You may make it contain in the range which does not impair an effect.
  • a commercially available product may be used as the polycarbonate resin.
  • the polycarbonate resin For example, 301-4, 301-10, 301-15, 301-22, 301-30 of “Caliver (registered trademark)” manufactured by Sumika Stylon Polycarbonate Co., Ltd. 301-40, SD2221W, SD2201W, TR2201 and the like.
  • thermoplastic resin layer When two or more types of (meth) acrylic resins are used in the thermoplastic resin layer, or when the (meth) acrylic resin is used in combination with another thermoplastic resin, the thermoplastic resin layer is formed. It is preferable to contain 50 parts by mass or more of (meth) acrylic resin per 100 parts by mass of the thermoplastic resin. As the thermoplastic resin other than the (meth) acrylic resin, a thermoplastic resin compatible with the (meth) acrylic resin is preferable.
  • thermoplastic resin layer does not substantially contain a vinylidene fluoride resin.
  • the film of the present invention is transparent when visually observed, and the total light transmittance (Tt) measured according to JIS K7361-1 is preferably 88% or more, more preferably 90% or more, and 60 ° C. This range is maintained even after 120 hours of exposure in an environment with a relative humidity of 90%.
  • the film of the present invention contains a (meth) acrylic resin and a vinylidene fluoride resin, and the haze measured according to JIS K7136 after exposure to an environment of 90% relative humidity at 60 ° C. for 120 hours is usually 2% or less, preferably It is 1.8% or less, more preferably 1.5% or less.
  • the film of the present invention has a relative dielectric constant at 3 V and 100 kHz measured by an automatic equilibrium bridge method in accordance with JIS K6911, usually 4.0 or more, preferably 4.1 or more.
  • the relative dielectric constant at 3 V and 100 kHz measured by the automatic equilibrium bridge method according to JIS K6911 is usually preferably 3.5 or more, 3.6 or more, more preferably 3.8 or more. is there.
  • the value of the relative dielectric constant is a value obtained by measurement performed before the film is exposed to a high temperature and high humidity environment.
  • the film of the present invention can be produced by molding the resin composition of the present invention by, for example, a melt extrusion molding method, a hot press method, an injection molding method, or the like.
  • a laminate may be produced by laminating a film obtained by molding the resin composition of the present invention by the above molding and a separately molded thermoplastic resin layer via, for example, an adhesive or an adhesive, It is preferable to produce a laminate by laminating and integrating the resin composition of the present invention and a (meth) acrylic resin by melt coextrusion molding.
  • the laminated body manufactured by melt coextrusion molding tends to be easily subjected to secondary molding as compared with the laminated body manufactured by bonding.
  • melt coextrusion molding for example, the resin composition of the present invention and (meth) acrylic resin are separately fed into two or three uniaxial or biaxial extruders and melt-kneaded, respectively, and then fed.
  • This is a molding method in which the film of the present invention and a thermoplastic resin layer are laminated and integrated through a block die, a multi-manifold die or the like, and extruded.
  • the obtained laminate is preferably cooled and solidified by, for example, a roll unit.
  • Another embodiment of the laminate of the present invention is at least one function selected from the group consisting of the above-mentioned film and at least one surface of the film, the anti-scratch, anti-reflection, anti-glare and anti-fingerprint.
  • the coating layer only needs to be laminated on at least one surface of the film, and does not necessarily need to be in contact with the film, and may be laminated via another layer.
  • a cured film described in JP2013-86273A can be used as the coating layer.
  • the thickness of the coating layer is preferably 1 to 100 ⁇ m, more preferably 3 to 80 ⁇ m, and even more preferably 5 to 70 ⁇ m. If it is thinner than 1 ⁇ m, it is difficult to express the function, and if it is thicker than 100 ⁇ m, the coating layer may be cracked.
  • the surface of the coating layer may be subjected to antireflection treatment by a coating method, a sputtering method, a vacuum deposition method, or the like.
  • a separately prepared antireflection sheet may be bonded to one side or both sides of the coating layer.
  • the antireflective sheet only needs to be laminated on at least one surface of the coating layer, and is not necessarily in contact with the coating layer, and may be laminated via another layer.
  • thermoplastic resin layer is abbreviated as B layer
  • coating layer is abbreviated as C layer
  • examples of the layer structure of the film and laminate of the present invention include the following (1) to (12). It is done.
  • a laminate having a structure represented by B layer / A layer / B layer can be produced as follows. This will be described with reference to FIG. First, a (meth) acrylic resin and a vinylidene fluoride resin can be mixed as a material for forming the A layer to obtain the resin composition of the present invention. Next, the resin composition is melted by the single screw extruder 2 and the thermoplastic resin is melted by the single screw extruders 1 and 3 as the material for forming the B layer.
  • a transparent conductive sheet can be obtained by forming a transparent conductive film on at least one surface of the film or laminate of the present invention.
  • a method of forming a transparent conductive film on the surface of the film or laminate of the present invention a method of directly forming a transparent conductive film on the surface of the film of the present invention may be used, or a plastic having a transparent conductive film formed in advance.
  • a method of forming a transparent conductive film by laminating a film on the surface of the film or laminate of the present invention may also be used.
  • the film base of the plastic film on which the transparent conductive film is formed in advance may be a transparent film that can form a transparent conductive film.
  • a transparent film that can form a transparent conductive film.
  • polyethylene terephthalate, polyethylene naphthalate, polycarbonate, An acrylic resin, polyamide, a mixture or laminate thereof can be exemplified.
  • the method for laminating a film, on which a transparent conductive film has been formed in advance, on the surface of the film or laminate of the present invention may be any method as long as it is free from bubbles and provides a uniform and transparent sheet.
  • a method of laminating using an adhesive that is cured by normal temperature, heating, ultraviolet light, or visible light may be used, or a transparent adhesive tape may be used for bonding.
  • a vacuum deposition method As a method for forming a transparent conductive film, a vacuum deposition method, a sputtering method, a CVD method, an ion plating method, a spray method, and the like are known, and these methods are appropriately used depending on a required film thickness. Can do.
  • the sputtering method for example, a normal sputtering method using an oxide target, a reactive sputtering method using a metal target, or the like is used. At this time, oxygen, nitrogen, or the like may be introduced as a reactive gas, or means such as ozone addition, plasma irradiation, or ion assist may be used in combination. If necessary, a bias such as direct current, alternating current, and high frequency may be applied to the substrate.
  • the transparent conductive metal oxide used for the transparent conductive film is indium oxide, tin oxide, zinc oxide, indium-tin composite oxide, tin-antimony composite oxide, zinc-aluminum composite oxide, indium-zinc composite. An oxide etc. are mentioned. Of these, indium-tin composite oxide (ITO) is preferable from the viewpoint of environmental stability and circuit processability.
  • a transparent conductive film it is formed by applying a coating agent containing various conductive polymers that can form a transparent conductive film and irradiating and curing with ionizing radiation such as heat or ultraviolet rays.
  • a coating agent containing various conductive polymers that can form a transparent conductive film and irradiating and curing with ionizing radiation such as heat or ultraviolet rays.
  • the method of doing etc. is applicable.
  • the conductive polymer polythiophene, polyaniline, polypyrrole, and the like are known, and these conductive polymers can be used.
  • the thickness of the transparent conductive film is not particularly limited, but when a transparent conductive metal oxide is used, it is usually 50 to 2000 mm, preferably 70 to 1000 mm. If it is this range, it will be excellent in both electroconductivity and transparency.
  • the thickness of the transparent conductive sheet is not particularly limited, and an optimum thickness can be selected according to the demand for the product specifications of the display.
  • the film or laminate of the present invention and the transparent conductive sheet containing the film or laminate can be suitably used as transparent electrodes for display panel face plates, touch screens and the like.
  • the film or laminate of the present invention can be used as a touch screen window sheet.
  • membrane or laminated body of this invention can use a transparent conductive sheet as an electrode substrate of a touch screen of a resistance film system or an electrostatic capacitance system.
  • a touch sensor panel having a touch screen function can be obtained by arranging the window sheet for touch screen or the touch screen on the front surface of a liquid crystal display, an organic EL display or the like.
  • the touch screen window sheet can be used as a substitute for a glass sheet disposed on the outermost surface of a liquid crystal display or an organic EL display.
  • the touch screen window sheet can also be used for a plasma display, a field emission display (FED), a SED flat display, electronic paper, and the like.
  • FIG. 2 shows a schematic diagram of a cross section of a general capacitive touch sensor panel using the film or laminate of the present invention and a transparent conductive sheet containing the film or laminate.
  • 11 is a window sheet made of the film of the present invention
  • 14 is a transparent conductive sheet containing the film or laminate of the present invention
  • 12 is an optical adhesive layer
  • 13 is a liquid crystal display device.
  • FIG. 3 is a schematic cross-sectional view showing an example of a liquid crystal display device to which the film or laminate of the present invention is applied.
  • the film or laminate 20 of the present invention can be laminated on the polarizing plate 21 via an optical adhesive, and this laminate can be disposed on the viewing side of the liquid crystal cell 23.
  • a polarizing plate is usually disposed on the back side of the liquid crystal cell.
  • the liquid crystal display device 25 is composed of such members.
  • FIG. 3 is an example of a liquid crystal display device and is not limited to this configuration.
  • Table 1 shows the (meth) acrylic resins used in Examples and Comparative Examples and their physical properties.
  • the Vicat softening point (VST) in Table 1 is based on the B50 method specified in JIS K 7206: 1999 “Plastics—Thermoplastic plastics—Vicat softening temperature (VST) test method”, and a heat distortion tester [Co., Ltd.] Measurement was performed using “148-6 series” manufactured by Yasuda Seiki Seisakusho. The test piece at that time was measured by press-molding each raw material to a thickness of 3 mm.
  • melt mass flow rate was measured in accordance with the method specified in JIS K 7210: 1999 “Plastics—Test methods for melt mass flow rate (MFR) and melt volume flow rate (MVR) of thermoplastics”. This JIS stipulates that poly (methyl methacrylate) -based materials are measured at a temperature of 230 ° C. and a load of 3.80 kg (37.3 N).
  • the weight average molecular weight (Mw) of the methacrylic resin was measured by gel permeation chromatography (GPC). To create a GPC calibration curve, use a methacrylic resin made by Showa Denko KK with a narrow molecular weight distribution and known molecular weight as a standard reagent, create a calibration curve from the elution time and molecular weight, and calculate the weight of each resin composition. Average molecular weight was measured. Specifically, 40 mg of resin was dissolved in 20 ml of tetrahydrofuran (THF) solvent to prepare a measurement sample.
  • THF tetrahydrofuran
  • Table 2 shows the vinylidene fluoride-hexafluoropropylene copolymer used in the examples, the vinylidene fluoride-trifluorochloroethylene copolymer and polyvinylidene fluoride used in the comparative examples, and their physical properties.
  • VDF indicates the content of a structural unit derived from vinylidene fluoride contained in vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-trifluorochloroethylene copolymer, or polyvinylidene fluoride.
  • HFP represents the amount of hexafluoropropylene contained in vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-trifluorochloroethylene copolymer, or polyvinylidene fluoride. Indicates the content ratio (mass%) of the derived structural unit.
  • CETF is included in vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-trifluorochloroethylene copolymer, or polyvinylidene fluoride. Of structural units derived from chloroethylene trifluoride It represents the mass%). VDF, HFP, and CETF were measured by NMR.
  • each copolymer was dissolved in N, N-dimethylformamide (DMF) -d7 so as to be 20 to 30 mg / ml, and the total number of times of observation was 19F, using an INOVA300 manufactured by Varian. Measurement was performed under the condition of a resonance frequency of 282 MHz.
  • DMF N, N-dimethylformamide
  • the weight average molecular weight (Mw) of vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-trifluorochloroethylene copolymer or polyvinylidene fluoride was measured by GPC.
  • Mw weight average molecular weight
  • polystyrene was used as a standard reagent
  • a calibration curve was created from the elution time and molecular weight, and the weight average molecular weight of each resin was measured.
  • 40 mg of resin was dissolved in 20 ml of N-methylpyrrolidone (NMP) solvent to prepare a measurement sample.
  • NMP N-methylpyrrolidone
  • As the measuring device two columns made by Tosoh Corporation, “TSKgel SuperHM-H” and one “SuperH2500” were arranged in series, and a detector employing an RI detector was used. .
  • Example 1 55 parts by mass of SUMIPEX (registered trademark) MM (manufactured by Sumitomo Chemical Co., Ltd.) and 45 parts by mass of PVDF copolymer A were dry blended and then used with a lab plast mill (20 mm granulator) manufactured by Toyo Seiki Seisakusho. The mixture was melt-kneaded at 260 ° C. to obtain composite pellets. Using a press molding machine, a film having a thickness of 800 ⁇ m was produced from the obtained composite pellet at a set temperature of 220 ° C. When the produced film was visually observed, it was colorless and transparent.
  • Example 2 A film having a thickness of 800 ⁇ m was prepared in the same manner as in Example 1 except that 50 parts by mass of SUMIPEX (registered trademark) MM (manufactured by Sumitomo Chemical Co., Ltd.) and 50 parts by mass of PVDF copolymer A were used. When the produced film was visually observed, it was colorless and transparent.
  • SUMIPEX registered trademark
  • MM manufactured by Sumitomo Chemical Co., Ltd.
  • Example 1 A film having a thickness of 800 ⁇ m was prepared in the same manner as in Example 1 except that KF polymer (registered trademark) T # 1300 (manufactured by Kureha Co., Ltd.) was used instead of PVDF copolymer A. When the produced film was visually observed, it was colorless and transparent.
  • KF polymer registered trademark
  • T # 1300 manufactured by Kureha Co., Ltd.
  • ⁇ Comparative example 2> A film having a thickness of 800 ⁇ m was produced in the same manner as in Example 1 except that PVDF copolymer B was used instead of PVDF copolymer A. When the produced film was visually observed, it was colorless and transparent.
  • Example 3 A film having a thickness of 800 ⁇ m was prepared in the same manner as in Example 1 except that SOLEF (registered trademark) 31508 (manufactured by Solvay) was used instead of the PVDF copolymer A. When the produced film was visually observed, it was colorless and transparent.
  • SOLEF registered trademark
  • 31508 manufactured by Solvay
  • Table 3 shows the amount of alkali metal (Na + K) contained in the obtained film.
  • the alkali metal content was measured by inductively coupled plasma mass spectrometry.
  • Table 3 shows the relative dielectric constant of each film at 3 V and 100 kHz measured by the automatic equilibrium bridge method in accordance with JIS K6911.
  • Example 3 The film
  • Example 4 As a methacrylic resin and a vinylidene fluoride resin, SUMIPEX MM and SOLEF21508 shown in Tables 1 and 2 were mixed in proportions shown in Table 4 to obtain a resin composition (A) that forms the intermediate layer (A). For the thermoplastic resin layers (B) and (C), SUMIPEX MH shown in Table 1 was used. The laminated body was manufactured with the following method using the apparatus shown in FIG. Referring to FIG.
  • the resin composition (A) was melted with a 65 mm ⁇ single screw extruder 2 (manufactured by Toshiba Machine Co., Ltd.) and SUMIPEX MH was melted with 45 mm ⁇ single screw extruders 1 and 3 (manufactured by Hitachi Zosen Corporation). I let you. Next, these are supplied to a three-type three-layer distribution type feed block 4 having a set temperature of 230 to 270 ° C. and distributed so as to have a three-layer structure, and then extruded from a multi-manifold die 5 (manufactured by Hitachi Zosen Corporation).
  • the obtained film-like molten resin 6 is sandwiched between a first cooling roll 7 (diameter 350 mm) and a second cooling roll 8 (diameter 450 mm) arranged opposite to each other, and wound around the second roll 8 while the second roll 8 is wound. And the third roll 9 (diameter 350 mm). Then, it wound around the 3rd cooling roll 9, it shape
  • the obtained laminate 10 had a total film thickness of about 800 ⁇ m and was colorless and transparent when visually observed.
  • Example 5 A laminate was obtained in the same manner as in Example 4 except that the thermoplastic resin layer was formed of Caliber (registered trademark) 301-30. Table 6 shows the resin composition content and layer structure. The laminate was colorless and transparent. Further, in the same manner as in Example 1, measurement of the relative dielectric constant of the obtained laminate and high temperature and high humidity exposure test were performed. The results are shown in Table 7.
  • Example 6 By using the film obtained in Examples 1 and 2 or the laminate obtained in Examples 4 and 5 as a window sheet for a display, a display device can be produced.
  • the film formed from the resin composition of the present invention has a high dielectric constant and can maintain transparency even when used for a long time. Therefore, it is used in smartphones, portable game machines, audio players, tablet terminals, and the like. It is useful as a window sheet for a touch sensor panel or a display device.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne une composition de résine contenant de 45 à 60 parties en masse d'une résine (méth)acrylique et de 40 à 55 parties en masse d'une résine de fluorure de vinylidène pour 100 parties en masse de la quantité combinée de la résine (méth)acrylique et de la résine de fluorure de vinylidène, ladite résine de fluorure de vinylidène étant un copolymère de fluorure de vinylidène et d'hexafluoropropylène qui contient de 65 à 90 % en masse d'une unité structurale dérivée du fluorure de vinylidène et de 10 à 35 % en masse d'une unité structurale dérivée d'un hexafluoropropylène.
PCT/JP2016/067145 2015-06-12 2016-06-08 Composition de résine, film, écran tactile et dispositif d'affichage WO2016199829A1 (fr)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
JP2017213771A (ja) * 2016-05-31 2017-12-07 住友化学株式会社 透明粘着剤付き樹脂積層体及びそれを含む表示装置
WO2022255253A1 (fr) * 2021-06-03 2022-12-08 株式会社クラレ Composition de résine à base de fluorure de vinylidène, article moulé et corps multicouche

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JP2005248177A (ja) * 2004-02-20 2005-09-15 Arkema 応力下で白化しないｐｖｄｆと一緒に共押出し可能な組成物
JP2013244604A (ja) * 2012-05-23 2013-12-09 Meihan Shinku Kogyo Kk タッチスクリーン用透明シート、透明導電シート及びタッチスクリーン
JP2014509789A (ja) * 2011-03-17 2014-04-21 エルジー・ケム・リミテッド 親環境太陽電池用バックシート及びその製造方法
WO2016088667A1 (fr) * 2014-12-01 2016-06-09 住友化学株式会社 Composition de résines, film et dispositif d'affichage

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
JP2005248177A (ja) * 2004-02-20 2005-09-15 Arkema 応力下で白化しないｐｖｄｆと一緒に共押出し可能な組成物
JP2014509789A (ja) * 2011-03-17 2014-04-21 エルジー・ケム・リミテッド 親環境太陽電池用バックシート及びその製造方法
JP2013244604A (ja) * 2012-05-23 2013-12-09 Meihan Shinku Kogyo Kk タッチスクリーン用透明シート、透明導電シート及びタッチスクリーン
WO2016088667A1 (fr) * 2014-12-01 2016-06-09 住友化学株式会社 Composition de résines, film et dispositif d'affichage

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017213771A (ja) * 2016-05-31 2017-12-07 住友化学株式会社 透明粘着剤付き樹脂積層体及びそれを含む表示装置
WO2017208884A1 (fr) * 2016-05-31 2017-12-07 住友化学株式会社 Stratifié de résine avec adhésif transparent, et dispositif d'affichage contenant celui-ci
WO2022255253A1 (fr) * 2021-06-03 2022-12-08 株式会社クラレ Composition de résine à base de fluorure de vinylidène, article moulé et corps multicouche

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